In situ evaluation of model copper-cast iron

canisters for spent nuclear fuel: a case of

microbiologically influenced corrosion (MIC)
N. R. Smart*1, A. P. Rance1, B. Reddy1, L. Hallbeck2, K. Pedersen2 and
A. J. Johansson3
The Swedish method for disposal of spent nuclear fuel in a deep geological repository (KBS-3)
relies on the stability of the granitic bed-rock and two engineered barriers: a copper-cast iron
canister and highly compacted bentonite clay. In order to develop a better understanding of the
internal corrosion processes that could take place if a leak were to occur in the outer copper
canister, five miniaturised copper cast iron canisters were installed at a depth of 450 m at the
A spo Hard Rock Laboratory, in Sweden. The experiments differed in the density of the
surrounding bentonite buffer, as well as in the number and position of leak points that were
introduced in the copper shell. Several electrochemical techniques (e.g. AC impedance, linear
polarisation resistance and electrochemical noise) were used to monitor the corrosion of different
components of the experiment. Copper specimens were installed for post-test evaluation of the
rate of general corrosion, localised corrosion and stress corrosion cracking (SCC). In addition,
mechanical and environmental parameters, such as surface strain, hydrostatic pressure, redox
potential, pH, water chemistry, dissolved gases, and microbial numbers, diversity, and activity
were measured regularly. After five years of in situ exposure one of the canisters was retrieved
and analysed to characterise and evaluate the corrosion processes that had occurred during the
experiment. Extensive sulphide production by sulphate reducing bacteria led to rapid corrosion of
iron, and the formation of iron sulphide deposits on the copper and iron electrodes disturbed the
electrochemical measurements. This paper describes the various analyses that were carried out
on the model canister and summarises the conclusions that can be drawn.
Keywords: Spent nuclear fuel, Radioactive waste disposal, Copper, Iron, Corrosion, In situ testing, Microbiologically influenced corrosion, Sulphate
reducing bacteria

This paper is part of a special issue on Long-Term Prediction of Corrosion Damage in Nuclear Waste Systems

Introduction to occur in the outer copper canister, five miniaturised,

To ensure the safe encapsulation of spent nuclear fuel
for geological disposal, the Swedish Nuclear Fuel and
Waste Management Company (SKB) has proposed a
technology that consists of an outer copper canister with
a cast iron insert, commonly referred to as the KBS-3
concept. This design relies on the stability of granitic
rock and two engineered barriers: a copper cast iron
canister and highly compacted bentonite clay. In order
to develop a better understanding of the internal
corrosion processes that could take place if a leak were
1
AMEC, B150 Harwell, Harwell Oxford, Didcot, Oxfordshire, OX11 0QB,
UK
2
Microbial Analytics Sweden AB, Molnlycke Fabriker 9, SE-435 35
Molnlycke, Sweden
3
SKB, Swedish Nuclear Fuel and Waste Management Co., Box 250 SE-
101 24, Stockholm, Sweden
*Corresponding author, email nick.smart@amec.com
model, copper-cast iron canisters were installed at the
beginning of 2007 at a depth of 450m at the A spo Hard
Rock Laboratory, which is located in the Baltic sea
archipelago in Sweden. The ambient temperature at this
location is y15uC throughout the year. The experiment
is named MiniCan and its detailed design is shown in
Fig. 1.
The experiments differed in the density of the
surrounding bentonite buffer, as well as in the number
and position of 1 mm pinholes that were deliberately
machined into the copper shell. Several electrochemical
techniques (e.g. AC impedance, linear polarisation
resistance and electrochemical noise) were used to
continuously monitor the corrosion of different compo-
nents of the experiment.14 In addition, mechanical and
environmental parameters, such as surface strain,
hydrostatic pressure, redox potential, pH, water chem-
istry, dissolved gases, and microbial numbers, diversity,

2014 AMEC Nuclear UK Limited

Published by Maney on behalf of the Institute
Received 18 February 2014; accepted 19 June 2014
548 DOI 10.1179/1743278214Y.0000000213 Corrosion Engineering, Science and Technology 2014 VOL 49 NO 6

a stainless steel support cage showing bentonite pellets
in annulus between inner and outer stainless steel filters
and inner void holding copper cast iron model canister;
b copper canister being lowered into support cage; c
inner cast iron components; d sensors and corrosion
samples (including copper cast iron sandwich speci-
men to investigate corrosion induced expansion)
mounted above model canister assembly, inside support
cage
1 MiniCan experiment
and activity were measured regularly.5 The copper
canister was made from oxygen-free phosphorous doped
(OFP) copper and the insert was made from cast iron.
Bentonite MX-80 clay was used. The support cage was
made from 316L stainless steel and the plastic support
table holding the electrodes and corrosion coupons was
made of nylon. The detailed design of the experiment is
described in reference1 and the set up and results
obtained to date are summarised in references.24 After
nearly five years of in situ exposure, one of the canisters
Corrosion Engineering, Science and Technology
Smart et al. Corrosion of copper-cast iron nuclear containers
(Experiment 3; bentonite y1?3 kg dm23 dry density,
1 mm defect at top and bottom weld) was retrieved and
analysed to characterise and evaluate the corrosion
processes that had occurred. Full details of the
procedure for removing the canister and analysing it
are presented in references;68 this paper presents and
discusses the key results from the post-test examination
of the retrieved container.
Experimental
During removal of the canister from the A spo labora-
tory the experiment was extracted from its borehole,
whilst minimising exposure to oxygen. It was placed into
a tightly sealed, water-filled and nitrogen-purged transfer
flask and transported to the UK for analysis in an inert-
gas purged glovebox. Once in the glovebox the experi-
ment was dismantled and sectioned and various samples
were prepared for analysis without exposure to the
atmosphere. Samples from the dismantled experiment
were analysed using a range of analytical techniques to
characterise the extent of any corrosion and to identify
the corrosion products formed, as follows:
(i) visual observation and photography: to assess
the extent of any corrosion
(ii) raman spectroscopy; to identify mineral phases
(iii) X-ray diffraction (XRD): to identify crystalline
mineral phases.
(iv) scanning electron microscopy (SEM) and energy
dispersive X-ray analysis (EDX): to examine the
morphology of deposits and to determine the
elemental composition of materials
(v) SEM/EDX: to evaluate if stress corrosion
cracking (SCC) had occurred on U-bend speci-
mens
(vi) X-ray photoelectron spectroscopy (XPS): to
determine the composition of very thin films
on the surface of specimens, with a surface
sensitivity of a few atomic layers
(vii) Fourier transform infra-red spectroscopy
(FTIR): to identify chemical bonds and func-
tional groups in the materials.
In addition, the following measurements were carried
out:
(i) profilometry: to determine the extent of any
localised corrosion of the copper canister
surfaces
(ii) analysis of dissolved hydrogen in copper: to
determine whether any hydrogen produced by
corrosion had entered the material
(iii) gravimetric analysis: to determine the integrated
corrosion rate of the metal coupons
(iv) diversity analysis and determination of the
numbers of microorganisms attached in bio-
films on the steel and copper surfaces.
Prior to removal of Experiment 3 from the borehole a
set of water samples was collected from the headspace
above the miniature canister and analysed for chemical
composition, microorganisms and dissolved gases.7
Results
When the support cage was extracted from the transfer
flask it was seen to have a shiny appearance, meaning
that the external surface of the stainless steel support
cage had not suffered from significant corrosion. The
2014 VOL 49 NO 6 549
Smart et al. Corrosion of copper-cast iron nuclear containers
2 MiniCan experiment 3 after removal from borehole at
spo: (left) copper model canister; (right) sensors and
A Although the specimen was crumbly and cracked its
corrosion coupons
striking feature about the appearance of all the
components inside the support cage when the lid was
removed was that they were all covered with a layer of
black deposit, as shown in Fig. 2.
The bentonite in the annulus of the support cage,
which was originally present in pellet form, had swelled
to a homogeneous mass, without any indications of the
original boundaries between the bentonite pellets or
channeling in the bentonite. No further analysis of the
bentonite was carried out, but samples were removed for
microbial analysis.7 The bentonite had the consistency
of butter, with some reddish staining in the bentonite.
Even though all surfaces were covered with a layer of
black material, the iron surfaces appeared to have a
thicker layer of black material on them than the copper
surfaces. There was significant, non-uniform blackening
of the surface of the canister and the blackening was
concentrated on areas facing the holes in the inner
cylinder of the support cage. In addition, there was a
black flaky material on the plastic support table holding
the electrodes and coupons. A short summary of the
main results from analysis of the surfaces of various
components in the experiment is given below.
Copper electrodes and coupons
SEM/EDX analysis showed mainly copper with small
quantities of iron, carbon, oxygen, silicon, sulphur,
chlorine, and calcium. Raman spectroscopy showed
predominantly non-crystalline material with possible
indications of graphitic carbon and mixed oxide/
sulphide species (possibly a mixed CuFeS2 phase).
These results are consistent with a thin film of copper
sulphur/oxygen superimposed in some areas with a layer
rich in iron, sulphur and silicon. The corrosion product
developed on copper specimens mounted outside the
steel cage, thus exposed directly to the borehole water,
was predominantly copper oxide, with only a trace of
sulphide present.
Copper weight loss specimen
SEM/EDX analysis of the weight loss specimen showed
a uniform coating of very small particles (typically
550 Corrosion Engineering, Science and Technology 2014
,5 mm) predominantly composed of copper and sul-
phur, with small quantities of iron, silicon, oxygen,
carbon, calcium, and chlorine. The gravimetric analysis
gave an integrated corrosion rate for copper of
0?150?02 mm year21.
Iron electrodes and coupons
Elongated black whiskers of material were observed
hanging vertically down from the cast iron weight loss
coupon and the cast iron electrodes. The whiskers, and
the corrosion products adhering to the cast iron
electrodes and coupons themselves, were found to be
mainly amorphous and EDX analysis showed a high
content of iron and sulphur. Raman analysis showed the
presence of graphitic carbon and possibly weak sulphide
peaks, and XRD analysis showed that the material was
amorphous. EDX analysis showed that the main
elements were iron, silicon, sulphur and oxygen.
Iron weight loss specimen
dimensions remained approximately the same as the
initial coupon. Raman analysis showed that the material
was amorphous, as shown by the broad peaks, with no
evidence for the common iron oxides. The broad Raman
peaks overlapped with the position expected for pyrite,
FeS2, but it was not possible to identify the species
present conclusively from the Raman spectra. In the
XRD analysis the only crystalline phase detected was
graphite, meaning that all metallic iron had been
corroded. The final weight of the coupon was 22% of
its starting weight, giving a cast iron corrosion rate of at
least 500 mm year21.
Black flaky material from support table
Raman and XRD analysis showed indications of Fe2O3,
carbonate, graphitic carbon and iron sulphide. The
material was amorphous. SEM/EDX analysis showed a
mass of closely compacted small crystallites (,5 mm), a
high concentration of iron, sulphur, silicon and oxygen,
and the flakes were approximately 0?1 mm thick. They
were probably formed by dissolution of iron from
electrodes and weight loss specimens and precipitation
as iron sulphide.
Copper canister with iron insert
No dimensional changes were measured compared with
the original design (to an accuracy of 0?05 mm) and
there were no signs of crevice corrosion around the O-
ring seal between the lid and body of the iron insert. The
simulated fuel channels inside the cast iron insert were
dry and showed no sign of corrosion. Flakes on the
outer surface were predominantly amorphous with a
trace of FeS (troilite) or CuFeS2 (chalcopyrite). The
results of the hydrogen analyses on two samples cut
from the canister were 0?594 ppm for a section cut from
the inner surface of the copper canister and 0?536 ppm
for the outer surface. Although the hydrogen content of
this specific copper material was not determined before
installation of the experiment, earlier batches of OFP
copper from the same manufacturer contained on
average 0?37 ppm (s50?14), and some batches had up
to 0?60 ppm hydrogen.9 This suggests that the hydrogen
content was largely unaffected by the corrosive exposure
during the experiment. The machined defects in the
copper canister had become blocked with corrosion
VOL 49 NO 6

product, but locally high rates of corrosion of the cast
iron insert were observed opposite the machined defects
in the copper canister, indicating high levels of microbial
activity in these areas.
Microorganisms and biofilms
The concentration of dissolved ferrous iron measured
inside the support cage had increased over the five year
test period, leading to a concentration of several 10 s of
mg L21. The concentration of sulphate had decreased,
with an accompanying increase in the numbers of SRB.
Cultivation of samples from water and biofilms on
various surfaces in the experiment revealed the presence
of sulphate reducing bacteria (SRB). On the canister
surface, the population exclusively consisted of SRB.
DNA analysis identified several species of SRB, includ-
ing Desulfovibrio ferrophilus, which is able to metabolise
metallic iron directly (using iron as an electron source).
Cultivable heterotrophic aerobic bacteria (CHAB) and
acetogenic autotrophes (AA) were present at the
beginning of the experiment, but they seem to have
disappeared during the subsequent years.5 The diversity
of the microbial populations fluctuated over time but
the total number of microbes present was relatively
constant.
Discussion
In order to analyse the results obtained by post-test
examination, it is helpful to briefly discuss the chemical
and biological environment inside the experiment. The
results from the microbial analysis7 show that there was
a significant difference between the microbial popula-
tions on the outer surface of the support cage, which was
exposed to the borehole water, compared to the
population on the surface of the copper canister, which
was exposed to the water inside the support cage. The
outer surface of the support cage had higher numbers of
CHAB than the surface of the copper canister, whereas
the surface of the copper canister had a very high
number of SRB but just a few CHAB. Both types of
bacteria were detected in the groundwater sampled from
within the Experiment 3 support cage, although the
number of SRB was higher. During the course of the
experiment the pH varied between 7?6 and 6?6, and
the concentration of Fe2z increased by more than one
order of magnitude. The concentration of SO422
remained nearly constant above 400 mg L21 during
20072010, but fell to 271 mg L21 in 2011, and the
sulphide concentration fluctuated below 0?1 mg L21.
Some oxygen was present in the near-field initially, since
the bentonite pore volume and other voids in the
experimental configuration contained air at installation
of the experiment (which might explain the presence of
some Fe2O3 in the Raman/XRD analysis of black flakes
on the support table). The redox potential in the
borehole fell from an initial value of y0 mV(SHE),
which indicates the presence of residual oxygen, to
2300 mV(SHE) within a few months, while the poten-
tial inside the support cage stabilised at around
2400 mV(SHE).3
Corrosion of copper and iron coupons
The copper electrodes were covered with a black
material, which appears to have originated from
corrosion of the iron components in the experiment
Corrosion Engineering, Science and Technology
Smart et al. Corrosion of copper-cast iron nuclear containers
(i.e. an ironsulphursilicon rich graphitic carbon
phase), but the underlying copper surfaces were covered
with a thin film of an unidentified mixed copper oxide
sulphide. The copper weight loss sample appeared to be
coated with a layer of small (i.e. ,5 mm) crystals of
copper sulphide, or a mixed ironcopper sulphide. The
formation of a layer of copper sulphide on the surface of
copper in the presence of SRB is well documented in the
literature.10
The weight loss measurement on the copper sample
gave an integrated corrosion rate of 0?150?02
mm year21. This is considerably lower than the corro-
sion rates measured by electrochemical methods,3 which
are considered to be erroneous due to the deposition of a
surface layer of conductive iron corrosion product
derived from the iron electrodes and coupons, and the
neighbouring cast iron insert. This phenomenon has
been observed by other workers.11 Corrosion rates
measured using the electrical resistance technique in
canisters not yet retrieved from the MiniCan experiment
are closer to the gravimetrically measured rate (0?25
0?39 mm year21).2,3 It should be noted that both the
copper and iron weight loss specimens were electrically
isolated from other metallic parts of the experiment, and
that the environment was aggressive due to the high
numbers of SRB inside the support cage, as well as in
biofilms on the canister. To that extent the experiment
represents a severe test of microbiologically influenced
corrosion (MIC) for the copper material, which may not
be representative of conditions for a copper canister
surrounded by highly compacted bentonite in the
repository.12
Corrosion experiments performed under anaerobic
laboratory conditions, using simulated groundwater
compositions, have shown that the abiotic anaerobic
corrosion rate of iron is of the order of ,1 mm
year21.13,14 However, the corrosion rate measured
gravimetrically in the MiniCan experiment was approxi-
mately three orders of magnitude higher and the
inevitable conclusion is that this increase in corrosion
rate was due to the large numbers and vigorous activity
of sulphate reducing bacteria (SRB) in the water filled
void inside the support cage of the experiment. SRB are
well known to cause accelerated corrosion rates10 of iron
based alloys, with the end product being iron sulphide
films. Even though the exact mechanism utilised by SRB
in the present case is unknown, there is a limited number
of possibilities. The possibility of iron as the electron
source for sulphate reduction according to reaction (1)
has some experimental support, however, the composi-
tion and stoichiometry of the iron sulphide depends on
the redox potential and pH (Ref. 10)
4FezSO4 2{ z4H2 O?3Fe(OH)2 zFeSz2OH{ (1)
The stoichiometry of reaction (1) suggests that solid
iron sulphide and iron oxide should form in similar
quantities*. This could be the case in the experiment at
hand, since even if iron sulphide seems to be the major
*According to reaction 1, the ratio of solid iron hydroxide and sulphide
should be 3 : 1. However, the stoichiometry of iron sulphide can undergo
alterations by long-term exposure to SRB.9 Also, the kinetic and/or
thermodynamic stability of solid iron hydroxide in reducing sulphidic water
is unclear to the authors, but is likely to affect the composition of the
corrosion products of iron.
2014 VOL 49 NO 6 551
Smart et al. Corrosion of copper-cast iron nuclear containers
3 a optical micrograph of outside cross-section of copper U-bend specimen and b selected part of outer surface of cop-
per canister near top hole
solid corrosion product formed, solid iron oxides/
hydroxides are observed and the concentration of
ferrous iron in the water inside the steel cage has
increased dramatically (from 0?82 mg L21 in 2007 to
49?6 mg L21 in 20117). SRB are able to metabolise
hydrogen to reduce sulphate to sulphide.15 Hydrogen
may be generated by the anaerobic corrosion of
iron;13,14 however, a recent study16 suggests that some
strains of lithotrophic SRB can use iron as a direct
electron source, without the need for intermediate
hydrogen formation. These strains were detected in
the MiniCan experiment.7 Another possibility is that
SRB oxidised dissolved organic material (or methane)
in order to reduce sulphate. The exact mechanism of
the bacterial sulphate reduction is still a matter of
investigation.
The form of attack of cast iron observed in the
MiniCan experiment is an example of graphitisation,17
which is common in the water industry where cast iron
pipes are used to transport water supplies. This results in
the conversion of the metallic structure to a weak porous
mass of corrosion product and graphite residue.
The conditions inside the MiniCan support cage are
conducive to SRB growth, because of the presence of
plenty of water, an abundant supply of sulphate and
hydrogen, the absence of oxygen and traces of organic
material in the bentonite. The conditions within
compacted bentonite, as would be used in the KBS-3
concept, would be less conducive to SRB activity
because of the lower water activity and lower supply
rate of sulphate.12,18
Corrosion morphology
None of the U-bend specimens installed showed any
signs of stress corrosion cracking (SCC) when examined
metallographically, i.e. no initiation of trans- or inter-
granular cracks could be observed with SEM (Fig. 3a).8
Optical microscopy and SEM revealed a partly rough
surface in agreement with earlier experiments with OFP
copper embedded in bentonite, in saline ground-
water.16,19 A striking feature of the copper shell is that
some areas of the surface were relatively unaffected by
corrosion, despite the long term exposure to saline
ground water. Figure 3b shows an area of the outer
copper surface that is partly covered with a crystalline
deposit (that was rich in iron and sulphur). Note that on
552 Corrosion Engineering, Science and Technology 2014
areas without this deposit it is still possible to see
machining marks, which is probably a reflection of the
low rate of general corrosion discussed above (0?15
0?02 mm year21).
Miniature canister
The analysis of components cut from the copper canister
showed the presence of a range of materials, including
crystals with a high concentration of copper and
sulphur. It was not possible to discern from the analysis
the exact stoichiometry of the crystals because the
analytical technique used, EDX, is semi-quantitative,
but there is a range of stoichiometric and non-
stoichiometric6,10 copper sulphides that could be present
on the surface of the canister and it is not possible to
determine the exact mineral composition from the
current dataset. The majority of the iron sulphide
deposited in the void inside the MiniCan experiment
appears to have originated from dissolution and
precipitation of iron from the iron corrosion coupons.
In summary, the experiment analysed shows that in a
deep granitic repository, the establishment of sulphate
reducing bacteria (SRB) can locally lead to rapid
corrosion of cast iron (500 mm year21). Despite the
presence and activity of SRB, the corrosion of copper
was slight. The establishment of SRB would be
supported by the presence of low density bentonite,
but may be restricted by the use of compacted bentonite.
Increased compaction will reduce the availability of
water, which is an essential requirement for the
proliferation of bacteria. Furthermore, increased com-
paction will expose the bacteria to high mechanical
stress that will eventually puncture and kill them. The
MiniCan in situ experiment is ongoing and two more
canisters are planned to be retrieved; one with highly
compacted bentonite and one without bentonite. The
post-test analysis of these canisters will give valuable
information about the role of the bentonite buffer and
its impact on microbiologically influenced corrosion.
Conclusions
A detailed analysis of MiniCan Experiment 3 has been
conducted under carefully controlled conditions and the
main conclusions from the investigation are as follows.
VOL 49 NO 6

1. The corrosion observed in the MiniCan experiment
was heavily influenced by the extensive activity of
sulphate reducing bacteria (SRB) in the groundwater-
filled headspace inside the support cage but above the
canister. This aqueous phase is not expected to occur
next to the canisters in the KBS-3 repository in the
presence of highly compacted bentonite.
2. After the five year exposure period, the cast iron
weight loss coupon was a mass of graphite and
amorphous iron oxide/silicon corrosion product. This
corrosion process for cast iron is commonly referred to
as graphitisation.
3. The corrosion rate of the cast iron was at least
500 mm year21, based on weight loss and electrochemi-
cal measurements.
4. The iron released into the groundwater through
corrosion had precipitated as a black deposit on all
surfaces inside the support cage; it was predominantly
composed of an amorphous iron sulphide, but it also
contained graphitic carbon and a silicon rich phase.
5. The integrated corrosion rate of the copper was
estimated to be 0?150?02 mm year21, on the basis of
weight loss measurements. This is considerably lower
than the corrosion rates measured by electrochemical
methods, which are considered to be erroneous due to
the deposition of a surface layer of conductive iron
corrosion product derived from the iron electrodes and
coupons, and the neighbouring cast iron insert. The
copper corrosion product was composed of a mixture of
copper oxide and copper sulphide.
6. There were no indications of localised corrosion
(i.e. pitting or stress corrosion cracking) of the copper
test specimens.
7. The outer dimensions of the retrieved copper
canister were measured and no changes from the initial
design dimensions were detected, meaning that no
expansion had occurred due to corrosion of the cast
iron insert. No expansion was observed in the copper
cast iron sandwich specimen either.
8. Copper sulphide crystals were observed on the
surfaces of the canister. The copper and cast iron
surfaces that were in close proximity (e.g. between the
cast iron insert and the copper canister, and between the
cast iron and copper pieces in the sandwich specimen)
had corroded less than fully exposed surfaces (e.g. the
weight loss specimen).
Acknowledgements
The authors gratefully acknowledge SKB for financial
support and the technical assistance provided by staff at
spo URL, and the University of Oxford Materials
the A
Characterisation Services for provision of analytical
services.
Corrosion Engineering, Science and Technology
Smart et al. Corrosion of copper-cast iron nuclear containers
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